Process of making catalytic material



' of oils. I

UNITED sTA'rns rerun Torsion.

' cmnron ELLIS, or monrcnam, NEW Juneau.

' 'rnocnss or MAKING ca'rALY'rIc newsman.

1,329,323. No Drawing.

To all whom z'tma concern:

Be it known t at I, CARLETON Ennis, a

.citizen of theUnited States, and a resident of Montclair, in-the countyof Essex and State of New Jersey, have invented'certain new and usefulImprovements in Processes of Making Catalytic Material, of which thefollowing is a specification.

. 'This invention relates to to the reduction of nickel nitrate, nickelnitrite or similar nickel salt of an acid of the nitrogen oxid groupunder regulated-reducjng conditions to yield active catalytic materialsuitable for use in the hardening Nickel nitrate is difiicult to reducein such a manner as to obtain a porous, finely divided, stronglycatalytic substance which nmiy be used for the hardening of oils.

' 'n""carrying out the operation according jto tfhe preferred form Iheat nickel nitrate in a reducing drum first in the presence of steamand then in contact with a mixture of steam and hydrogen. The nickelnitrate heating effect that sintering would occur,

forming a nickel material which would be too coarse to have usefulcatalytic properties. On heating in the presence of steam however thenickel nitrate breaks down uniformly leaving a porous finely-divided:

product which subsequently is reduced with hydro en or' other reducinggas to form metallic nickel or other catalytic powdered nickel body. I

In carrying out the invention nickel nitrate, nitrite or similarinorganic salt-of nickel capable, on heating or reduction, of yielding acatalytic material, is preferably pulverized and heated in a revolvingdrum. In the first stages water may be evolved if the product has notfirst been well dried. After this water. has been expelled steam may beadmitted and subsequently a mixture of steam and carbon monoXid,hydrogen or other reducing gas, the temperature being carried to between300'and 400 C. Prefer Speqificaflcn of Letters Patent.

a method of producing a catalyzer and relates especially drogen or otherreducing gas-is present without dilution with any inert or extending gasproximately at 200 C. From there on con-- siderable reaction will takeplace when hydrogen or other combustible gas is used without a diluentand the local heating which may be caused is likely to sinter the cat alyzer as stated. In addition there isf-tlie? possibility of explosiondue toini'xturescf the nitrous oxid fumes with hydrogen or otherreducing gas employed Hence in the PatentedJan. 2'7, 1920. Applicationfiled January 31, 1919. Serial 110.274357.

present invention it is an objectto regulate"= the reducing conditionswith respect td-th'e evolution of nitrous fumes so that local heating ofan objectionable character is'i'avoided and a tendency toexplosions'minimized.

1 The operation may be carried out by, for

example, drying nickel nitrate in an open pan until substantially freefrom moisture and then grinding to a fine powder. This is placed in arevolving drum or preferably an elongated cylinder which infact may befitted with conveyers so as tofeed the product progressively along thecylinder so as to afford a continuous process of reduction.

However in the simpler form of operation the nickel nitrate is agitatedin a closed re,- ceptacle and the atmosphere in the receptacle ismodified from time to time beginning preferably with steam or-a mixtureof.

steam and a small amount ofghydrogen or other reducing gas andincreasing the latter gradually as the temperature is rai' s'ed toa;final temperature of 350 or 400 (1; at the end pure reducing gas beingpassed through the receptacle. When nickel nitrate is grad-' uallyheated in a current of hydrogen gas a particularly violentreaction-occurs at about 240, the mass glowing and .sintered materialbeing produced. Great care should be exercised in passing this point inthe reducing operation to avoid such a sudden and violent reaction whichis fatal to the success of the operation. To obtain the K catalyzer innon-pyrophoric form nitrogen may subsequently be introduced into there-= ceptacle to wash out the hydrogen. In lace of reducing gas areducing vapor sue as the vapor of alcohol, gasolene and the like may beemployed. Ammonia also may be .used as a redilcing agent. In someinstances and used as a hardenin fairly non-pyrophoric.

appropriate liquids may also be used asreducing agents, in anunvaporized condltion. The expression bathing fluid, as used in thisapplication, is intended to cover gases, vapors and liquids. Thereceptacle allowedto'cool and when cold the catalyzer is withdrawn andmay be introduced into 0 11 catalyzer. It s n a second modifi cation ofthe invention, nickel nitrate is mixed with molten paraflin wax andgradually heated while being stirred. TlllS operation is convenientlyconducted in a deep vessel having a cover or lid which may be Thetemperature is gradual 340 0., and is held at this point for half anhour or more. The resulting product is a deep velvety black masscontaining partiall cracked parafiim and. a black "owder whic seems toconsist entirely or su stantially of -metallic nickel. 'The paraflin canbe re-' moved from the. mass by settling and washing with benzol orgasolene, if desired.' The remaining powder constituting the catalyzeris a peculiar one, it is magnetic, has a deep black color, a mossyaprance and is usually substantially free om metallic luster.

It seems to consist of a black amorphous nickel material. It isnon-pyrophoric and in its preferred form, this product is not readilyoxidized. It may be exposedto the air for a considerable period and showlittle or no deterioration.

Preferably no hydrogen or other reducing s is introduced into theparafiin wax durmg the operation The employment of paraflin or similarmaterial, heated to a tem-' perature of about 340? 0., is not broadlyclaimed in the present application, but in my co nding application,Serial No. 314,738, filed August 1, 1919.

T0 recapitulate the invention embraces the treatment of nickel nitrateor analogous inorganic salt of nickel or for that matter nickel andcobalt'or cobalt and other metals of like character capable of acting aseffective hydrogen carriers inthe hardening of fatty oils, underregulated reducing conditions which prevent violent reaction with thereducing gas or reducing agent thereby preclding sintering of theproduct obtain i Y it decomposes An advantage in using nickel nitrate isthat it is a comparatively cheap salt of.

nickel being for example substantially cheaper than nickel formats- Alsoit may be produced readily in a state of purity, free .from catalyzerpoisons. Also when heated ving ofi gases which disappear from the eld ofreaction without leaving any residue. For these reasons nickel nitrateis a desirableraw material for making the catalyzer and the presentprocedure enables its production in an effective.

manner. v I 7 What I claim is 1. The process of making a catalyzersuitable for-hardening oils which comprises exposing nickel nitrate to areducing atmosphere in the presence of steam whereby re duction takesplace without violent reaction and sintering, thereby yielding finelydivided catalytic material of anactive char'acter.

2. The process of making a catalyzer suitable for hardening oils whichcomprises exposing raw catalytic material comprising nickel nitrate tothe action of hydrogen and steam at an elevated temperature Wherebreduction of the nitrate to finely divided catalytic material isobtained without violent reaction and sintering.

3. The process of making a catalyzer suitable, for hardening oils whichcomprises heating raw catalytic material containing nickel nitrate in areducing atmosphere which durin the initial stages of reduction containsa dlluting agent whereby finely divided catalytic material is obtainedwithout violent reaction and sintering.

4. The rocess of making a catalyzer suitable for ardening oils whichconsists in heating catalytic raw material containing nickel nitrate ina reducing atmosphere whereby reduction to" catal ic material takesplace and during. the initial stages of the reduction in diluting thereducing atmosphere by a non-reducing agent whereby violent reaction andsintering is avoided.

5. The process of makin a catalyzer suitable for the hardening 0 oilswhich comprises heating catalytlc raw material .containing a nickel saltof an acid of the nitrogen oxid group in an atmosphere of hydrogen andin introducing aquantity of steam during the initial stages of reductionin order to avoid sudden and violent reaction of the said nitrate withthe hydrogen, and in finishing the reduction with pure hydrogen.

6. The process of making a catalyzer suitable for ardening oils whichconsists in heating catalytic raw material containing.

nickel united with an acidof the nitrogen oxid group in a strongreducing atmosphere and in introducin a quantity of a diluting I agentduring the initial stages of the heating in order to avoid sintering ofthe nickel terial suitable for use in hydrogenating operations, whichcomprises heating a. raw

material containing nickel united with an acid containing anitrogen-oxygen group, in a bathing fluid having a reducing powersufiiciently great to reduce such nickel material, and maintaining thetemperature throughout the operation at not above 400 ing of the productis produced by heat generated by oxidation of the constituents of suchbathing fluid, by the oxygen of the nickel compound.

cAItLEToN- ELLIS.

(1., so that no substantial amount of sinter

